Preparation and characterization of chitosan/graphene oxide composites for the adsorption of Au(III) and Pd(II).

In this work, graphene oxide (GO) was firstly prepared, following by element analysis. Glutaraldehyde cross-linked chitosan (GCCS) and chitosan/graphene oxide (CSGO) composite with three different amounts of GO (5 wt%, 10 wt% and 15 wt%) were also prepared for the adsorption of Au(III) and Pd(II) in aqueous solution. The properties of the adsorbents were investigated by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and surface area analysis. Batch adsorption studies were carried out. The adsorption of Au(III) and Pd(II) onto CSGO composites was optimum at pH 3.0-5.0 for Au(III) and pH 3.0-4.0 for Pd(II), which was much wider than that of GCCS. The adsorption isotherms obeyed the Langmuir isotherm models for the adsorption of Au(III) and Pd(II). Chitosan with 5 wt% graphene oxide (CSGO(5)) composite had the largest adsorption capacity for Au(III) and Pd(II) compared with the other prepared adsorbents, where the maximum adsorption capacity were 1076.649 mg/g for Au(III) and 216.920 mg/g for Pd(II), respectively. The adsorption kinetics of Au(III) and Pd(II) onto CSGO(5) followed a pseudo-second-order kinetic model, indicating that the chemical adsorption was the rate-limiting step. Thermodynamic parameters, such as Gibbs energy (ΔG°), enthalpy (ΔH°), and entropy (ΔS°), were calculated, showing that the adsorption of Au(III) and Pd(II) onto CSGO(5) were spontaneous, endothermic and feasible. The desorption studies of Au(III) and Pd(II) onto CSGO(5) showed that CSGO(5) can be used repeatedly without significantly changing its adsorption capacity and desorption percentage after 3 cycles. Besides CSGO(5) was successfully applied for the determination and separation of Au(III) and Pd(II) in ore samples.

Determination of nitroanilines in hair dye using polymer monolith microextraction coupled with HPLC.

In this study, a novel method for the determination of nitroanilines in hair dye samples has been developed based on poly(methacrylic acid-co-ethylene glycol dimethacrylate) monolith microextraction (PMME) and high-performance liquid chromatography (HPLC) analysis. Four nitroanilines, p-nitroaniline (PNAL), m-nitroaniline (MNAL), o-nitroaniline (ONAL), and 2,4-dinitroaniline (DNAL), are studied as representatives. To obtain optimum extraction efficiency, several experimental parameters including sample flow rate, sample volume, sample pH, and eluent flow rate have been investigated. Under the optimal experimental conditions, the linear regression coefficients of the standard curves are greater than 0.9990. The limits of detection for p-nitroaniline, m-nitroaniline, o-nitroaniline, and 2,4-dinitroaniline are 0.012, 0.008, 0.018, and 0.005 µg/mL, respectively. The intraday and interday relative standard deviations are less than 3.1 and 5.4%, respectively. The proposed method is simple, rapid, sensitive, and competent when used for the determination of nitroanilines in hair dye samples and the accuracy is assessed through recovery experiments.

Ultrasonic extraction and separation of anthraquinones from Rheum palmatum L.

The ultrasonic nebulization extraction (UNE) was developed and applied to extract anthraquinones (emodin, aloe-emodin and rhein) from Rheum palmatum L. Several parameters of UNE, including type of extraction solvent, concentration of extraction solvent, volume of extraction solvent, extraction time and ultrasonic power, were studied and the optimized parameters were selected. The operation conditions of micellar electrokinetic capillary chromatography (MEKC) were also studied. Under the selected conditions, contents of emodin, aloe-emodin and rhein obtained from different cultivated areas of R. palmatum L. were 1.08-2.04 mg/g, 0.65-1.16 mg/g and 0.70-2.90 mg/g, respectively. The relative standard deviations (RSDs) for emodin, aloe-emodin and rhein were 1.3-2.4%, 1.9-4.7% and 1.3-3.9%, respectively. Compared with maceration extraction (ME), reflux extraction (RE), stirring extraction (SE) and ultrasonic extraction (UE), the proposed method was more efficient, faster and easier to be operated and lower equipment costs and lower extraction temperature were required. The results indicated that UNE was a good alternative method for extracting anthraquinones from R. palmatum L. Compared with traditional extractions, the proposed extraction has a potential in on-line sampling, especially when the gas is used as the carrier of sample.

Determination of total flavonoids in Scutellaria barbata D. Don by dynamic ultrasonic extraction coupled with on-line spectrophotometry.

A dynamic ultrasonic extraction (DUE) coupled with on-line detection by spectrophotometry is proposed for the determination of total flavonoids (calculated against scutellarin) in Scutellaria barbata D. Don. The extraction was performed in a common self-made extraction vessel put in an ultrasonic bath and a peristaltic pump was used to deliver the extraction solvent. Several experimental parameters of DUE, including flow rate and concentration of extraction solvent, ultrasonic power and sample amount, were optimized. In this work an on-line method was provided with the advantages of minimum sample amount (5 mg), on-line monitoring the extraction process and time saving (12.5 min). Compared with off-line method, the proposed method would be more convenient for obtaining continuous measurements and rapid optimization of the extraction process.

[Photocatalysis characterization of titanium dioxide supported on natural clinoplilolite].

This paper studied preparing photocatalyst supported on natural clinoplilolite, photocatalysis degrading to methyl orange solution as photocatalysis function test, solar as light resource, explored the synthesize condition and affect factors of its catalysis activity. The capability of catalyst was evaluated by decolor rate and COD removal rate. The samples was described by XRD, IR and specific surface area. Studied result showed that catalyst prepared by combination of tetrabutyl titanate and natural clinoplilolite dryed under 120 degrees C for 6 hours then calcined under 200 degrees C had the best photocatalysis activity. Degrading rate of methyl orange solution increased with the quantity of TiO2/zeolite and additional oxidant H2O2 increasing, but superfluous H2O2 can also restrain the photocatalysis activity of titanium dioxide supported on clinoplilolite. Methyl orange solution had the best degrading rate as pH value between 2 to 5.